CN105154175A - Anti-wear agent for lubricating oil and preparation method thereof - Google Patents
Anti-wear agent for lubricating oil and preparation method thereof Download PDFInfo
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- CN105154175A CN105154175A CN201510453838.0A CN201510453838A CN105154175A CN 105154175 A CN105154175 A CN 105154175A CN 201510453838 A CN201510453838 A CN 201510453838A CN 105154175 A CN105154175 A CN 105154175A
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Abstract
The invention discloses an anti-wear agent for lubricating oil and a preparation method thereof. The anti-wear agent comprises modified carbon nano-tubes, modified nano-copper, POSS-MA-PEG (polyhedral oligomeric silsesquioxane -methacrylisobutyl-polyethylene glycol) and an oil-based solvent. The anti-wear agent can be used for enhancing the oil film strength, reducing the friction coefficient and realizing self-repairing of worn positions, and has functions of conserving energy, reducing emission, improving power and the like. The anti-wear agent can be well dispersed in various lubricating oils, has a stable oxidation performance, and is applicable to solution to friction, abrasion and maintenance problems of gasoline and diesel vehicle engines under multiple working conditions.
Description
Technical field
The present invention relates to a kind of anti-wear agent technical field, more specifically, the present invention relates to a kind of lubrication oil antiwear agent and preparation method thereof.
Background technology
Lubricating oil is mechanical movement and safeguards indispensable integral part.Along with the raising day by day of the working parameter such as load, speed, temperature of modern machinery and equipment, in lubricating oil, original low friction compound and anti-wear agent can not meet the requirement of its anti-wear and wear-resistant performance completely.In order to make up the defect of lubricating oil, usual employing adds lubricity and the wear resistance of the method raising lubricating oil of lubricating oil additive, as added multiple organic or inorganic mixture, liquid state or solid-state additive, it forms one deck liquid film by physics or chemisorption or chemical reaction, improve the supporting capacity of liquid film, reduce frictional coefficient.Since the nineties in 20th century, along with people are to the further investigation of nanomaterials and nanotechnology, find that nanoparticle has showed the frictional behaviour of a lot of excellence at lubricating area, the nano lubricating oil additive made with these nanoparticles can make the anti-attrition abrasion resistance of lubricating oil be greatly improved.
Therefore, developing a kind of high performance lubrication oil antiwear agent to strengthen oil film strength, reduce frictional coefficient and realize selfreparing, is the problem that those skilled in the art's common need are all the time captured.
Summary of the invention
In order to solve the problem, the invention provides a kind of lubrication oil antiwear agent and preparation method thereof.
In order to realize foregoing invention object, this invention takes following technical scheme:
A kind of lubrication oil antiwear agent, described anti-wear agent is prepared from by comprising following raw material:
Modified Nano copper 100
Modified carbon nano-tube 36 ~ 60
POSS-MA-PEG20~55；
Described modified carbon nano-tube is the carbon nanotube of polyisobutene modification; The molecular structural formula of described POSS-MA-PEG is:
Wherein, R is the one in phenyl, isobutyl-, cyclopentyl and cyclohexyl, and n is 70 ~ 130, R
1for the one in hydroxyl, amino and carboxyl.
In one embodiment, in described POSS-MA-PEG, R is phenyl or cyclopentyl.
In one embodiment, in described raw materials, also comprise the oil-based solvent of 5 ~ 25 weight parts, described oil-based solvent is selected from one or more in various lubricating oil and base oil.
In one embodiment, described modified Nano copper is the nano-particle of copper through benzothiazole compound in-situ-surface modifying.
In one embodiment, described benzothiazole compound is selected from
In one.
In one embodiment, in described modified Nano copper, the particle diameter of nano-particle of copper is 2 ~ 50nm.
In one embodiment, the caliber of described modified carbon nano-tube is 20 ~ 30nm.
Another aspect provides the preparation method Wu Ji – organic composite macromolecular flocculation agent, modified Nano copper, modified carbon nano-tube, POSS-MA-PEG and oil-based solvent are fully uniformly mixed by weight, and heat at 35 ~ 45 DEG C and be incubated 20 ~ 45min, to obtain final product.
In one embodiment, in described preparation method, temperature is 40 DEG C and is incubated 30min.
In one embodiment, described lubrication oil antiwear agent is used in lubricant products.
Be easier to understand the above-mentioned of the application and other features, aspect and advantage with reference to following detailed description.
Embodiment
More easily present disclosure can be understood with reference to the detailed description of following preferred implementation method of the present invention and the embodiment that comprises.Can mention a large amount of term in following specification sheets and claims, these terms are defined as following implication.
Singulative comprises plural number and object is discussed, unless clearly indicated in addition in context.
" optional " or " optionally " refers to that the item that describes thereafter or event can occur or not occur, and this description comprises situation that event occurs and the situation that event does not occur.
Quantity modified in approximate term in specification sheets and claims, represents that the present invention is not limited to this concrete quantity, also comprises close to this quantity acceptable and can not cause the part of the correction of the change of relevant basic function.Accordingly, modify a numerical value with " approximately ", " about " etc., mean and the invention is not restricted to this exact numerical.In some example, approximate term may correspond to the precision of the instrument measuring numerical value.In present specification and claims, scope limits and can combine and/or exchange, if do not illustrate that these scopes comprise contained all subranges therebetween in addition.
In order to solve the problem, the invention provides a kind of lubrication oil antiwear agent, described anti-wear agent is prepared from by comprising following raw material:
Modified Nano copper 100
Modified carbon nano-tube 36 ~ 60
POSS-MA-PEG20~55；
Described modified carbon nano-tube is the carbon nanotube of polyisobutene modification; The molecular structural formula of described POSS-MA-PEG is:
Wherein, R is the one in phenyl, isobutyl-, cyclopentyl and cyclohexyl, and n is 70 ~ 130, R
1for the one in hydroxyl, amino and carboxyl.
Term described in the present invention " modified Nano copper " is through the nano-particle of copper of organic compound in-situ-surface modifying.Nano-particle of copper is as a kind of soft metal, owing to having the excellent specific properties such as shearing force is low, ductility good, fusing point is low, thus there is well wear-resistant, antifriction performance, thus have broad application prospects in the lubrication, reduction frictional wear, raising engine power performance etc. of engine.But, there is high surface and chemically active nanoparticle is non-oil-soluble substance, and wettability is bad, stores at lubricating oil and be difficult to keep for a long time dispersion stabilization because easily reuniting in use procedure, and may because of generation oxygen
Change and rotten or lost efficacy, which has limited its application in lubricating oil, is such additive problem demanding prompt solution of Developing Application.For solving the problem of the dispersion stabilization of nano-particle of copper in oil-dissolving solvent, the general method adopting organic compound in-situ-surface modifying nano-particle of copper.Usually organic compound used be Acidic phosphates and salt, alkyl dithionic acid and salt thereof,
And benzothiazole compound.
Term described in the present invention " benzothiazole compound " is the important nitrogen heterocyclic containing the extreme-pressure anti-wear active element such as N, S of a class, lone-pair electron containing non-Cheng Jian in its molecular structure, empty d track that is easy and metal forms coordinate bond, by chemistry and physical action in metallic surface absorption film-forming, and the adsorption film of the more microscler one-tenth of chain on heterocycle is thicker, in friction process, be also easy to metallic surface simultaneously form chemical reaction film, and show good synergy; In addition, the phenyl ring in molecule and backbone can not only improve the thermostability of molecule, can also improve its oil soluble, thus make benzothiazole compound show good tribology, the anti-corruption of antioxygen and the over-all properties such as composite.What benzothiazole compound can introduce long-chain by active amino or sulfydryl improves its frictional behaviour containing O group or the long chain alkyl group containing O, and wherein O generally can occur with forms such as hydroxyl, carboxyl, ketone group, ester groups.The lone-pair electron and metallic surface positive charge point effect formation reaction film that one deck adsorption film and the S atom that is positioned at 1 have are formed in metallic surface, the common frictional behaviour improving oil product containing the strong coordination ability of O, S, N in the benzothiazole compound of O; Benzothiazole compound not containing O in the long-chain introduced, a pair lone-pair electron that its S atom being positioned at 1 still has can with frictional metal surface reaction formation reaction film, and the slightly weak atom N liquid of Electron Affinities and coordination ability can form adsorption film in metallic surface, thus improve the frictional behaviour of oil product.
In the present invention, term used " modified carbon nano-tube " refers to what carbon nanotube and polymkeric substance prepared through blending and modifying.Carbon nanotube, has another name called Baji-tube, and be that to have radial dimension be nanometer scale to one, axial dimension is micron dimension, the One-dimensional Quantum material of the special construction that pipe two ends are all sealed substantially.Carbon nanotube forms the coaxial pipe of several layers to tens of layers primarily of the carbon atom in hexagonal array, and keep fixing distance between layers, about 0.34nm, diameter is generally 2 ~ 20nm.Carbon nanotube can be regarded that graphene sheet layer is curling as and form, therefore can be divided into according to the number of plies of graphene film: Single Walled Carbon Nanotube and multi-walled carbon nano-tubes, multi-walled carbon nano-tubes is when starting to be formed, be easy between layers become Trapping Centers and catch various defect, thus multi-walled pipes be covered with usually the same defect of duck eye.Compared with multi-walled pipes, the distribution range of single-walled pipe diameter is little, and defect is few, has higher uniformity consistency.Single-walled pipe representative diameter is at 0.6 ~ 2nm, and multi-walled pipes innermost layer can reach 0.4nm, the most slightly can reach hundreds of nanometer, but typical caliber is 2 ~ 100nm.Carbon nanotube can be divided into three types according to its constitutional features: armchair nanotubes, zigzag nanotubes and chiral nanotubes.Carbon nanotube has good mechanical property, and CNTs tensile strength reaches 50 ~ 200GPa, and be 100 times of steel, density but only has 1/6 of steel, at least high than an ordinary graphite fiber order of magnitude; Its Young's modulus can reach 1TPa, suitable with adamantine Young's modulus, is about 5 times of steel.For the carbon nanotube of solid wall with ideal structure, its tensile strength is about 800GPa.Although the structure of carbon nanotube and the structural similitude of macromolecular material, its structure is much more stable than macromolecular material.Carbon nanotube is the material with most high specific strength can prepared at present.If with Other Engineering material for matrix and carbon nanotube make matrix material, composite material exhibits will can be made to go out good intensity, elasticity, fatigue resistance and isotropy, bring great improvement to the performance of matrix material.Modified carbon nano-tube in the present invention adopts polyisobutene and carbon nanotube with carrying out Homogeneous phase mixing according to weight part 60 ~ 95,5 ~ 45 respectively, and employing is ground or ultrasonic mode carries out dispersion 20min, and heat insulationly adds temperature control at 50 DEG C.
In of the present invention, term used " POSS-MA-PEG " is prepared via a step amidate action and a step esterification by aminopropyl POSS, maleic anhydride and modified poly (ethylene glycol).
Term described in the present invention " aminopropyl POSS " refers to that the sole active radicals R on POSS monomer is aminopropyl.Described term " POSS " refers to that cage-type silsesquioxane (PolyhedralOligomericSilsesquioxane is called for short POSS) is the hybrid molecule of a cage-like shape structure, and its skeleton symbol is (RSiO
1.5) n, wherein n is generally 6,8,10 or 12, and most widely used be hexahedron oligomeric silsesquioxane (T
8), namely n is the POSS molecule of 8.T
8class POSS molecule has the cubes cage structure of high degree of symmetry, and Si atom is positioned at cubical eight drift angles, is connected with O atom, the inorganic skeleton that to form with Si-O-Si nanostructure be core.T
8in class POSS, adjacent S i element spacing is 0.53nm, and organic group spacing is 1.5nm.This nanometer size effect and inorganic framework kernel, can provide good thermotolerance, oxidation-resistance, intensity and hardness for material.Its periphery is surrounded by organic group R, and these organic groups can be some active groups such as hydrogen base, vinyl, amino, also can be the inertia groups such as cyclohexyl, cyclopentyl, isobutyl-, phenyl.The POSS molecule containing different R group can be synthesized, to meet the demand of multiple reaction conditions and polymer performance by molecular designing.From the angle of molecular designing, POSS achieves organic phase from structure and combines with covalent linkage with inorganic phase, is an a kind of novel organic inorganic hybrid material.In this kind of material, by being evenly distributed in whole material after strong chemical bonds between inorganic phase characteristic (such as thermostability and oxidation-resistance) and organic phase characteristic (such as processibility and hardness are high), overcome the reunion of inorganic particulate and the weak problem of two interphase interface bonding forces, the polymkeric substance of formation shows mechanical property and the thermomechanical property of enhancing; In addition, it can be formed at lower temperature and gentle electrochemical conditions, and product is even, stable, good dispersity; Many conventional organic reagents can be dissolved in.
The method of synthesis POSS and derivative thereof has a variety of, and the reaction raw materials according to adopting can be divided into four large classes:
1) hydrolytic condensation method: namely first generate new Si-O-Si key, and then form cage structure, reacting the raw material adopted is XSiY
3type monomer, wherein X is chemical stability group, and as methyl, phenyl or vinyl etc., Y is then high reactivity group, as chlorine atom, through base or alkoxyl group etc., XSiY
3type reaction monomers can be linear, ring-type or polycyclic siloxanes.
2) T7 closed loop method, i.e. T7 and XSiY
3complete condensation forms the cage type hexahedron structure of POSS.
3) substituting group changes method, namely on the basis not changing the Si-O-Si key that oneself exists, changes the substituting group on Si atom, thus obtains the derivative of POSS (especially cage type POSS).Substituting group used have methyl alcohol, phenol, alkoxysilane, chlorosilane, epoxy derivative, the tenth of the twelve Earthly Branches purport, fluoroalkane, halogenide, isocyanic acid cruel, methacrylic vinegar, propylene vinegar, alkane, naphthenic hydrocarbon, eyeball, norbornylene, alkene, unicorn, silane, silanol and vinylbenzene etc.
4) ((CH
3)
4n)
8si
8o
20alkylation process, i.e. ((CH
3)
4n)
8si
8o
20the target product of desired structure is obtained by alkylated reaction.
The POSS base class polymkeric substance formed by copolyreaction, according to the number of the active group in eight organic substituent groups on POSS monomer, roughly POSS base class polymer materials can be divided into three major types: the first kind is " Star Network " structure, namely POSS cage contains the polymerisable functional group of two or more, once with organic monomer copolymerization, formed network structure; Equations of The Second Kind is " bead type " structure, and namely POSS cage contains two polymerisable functional groups, after copolymerization, POSS cage structure is gone here and there in polymer chain as pearl; 3rd class is " suspended pattern " structure, namely POSS cage only has a polymerisable functional group, and after copolymerization, POSS cage is suspended on polymer chain.
The copolymerization process of POSS base class polymkeric substance mainly contains: addition polymerization, general radical polymerization, atom transfer radical polymerization, polycondensation, ring-opening metathesis polymerization and polycoordination etc.
Term described in the present invention " PEG " has R
1(CH
2cH
2o) nCH
2cH
2r
1the polymkeric substance of structure, wherein R
1for the one in hydroxyl, amino or carboxyl.
In one embodiment, in described POSS-MA-PEG, R is phenyl or cyclopentyl.
In a preferred embodiment, in described POSS-MA-PEG, R is phenyl, R
1for amino.
In one embodiment, in described raw materials, also comprise the oil-based solvent of 5 ~ 25 weight parts, described oil-based solvent is selected from one or more in various lubricating oil and base oil.
In the present invention, term used " oil-based solvent " is mineral oil or synthetic oil.
In one embodiment, described modified Nano copper is the nano-particle of copper through benzothiazole compound in-situ-surface modifying.
In one embodiment, described benzothiazole compound is selected from
In one.
In one embodiment, in described modified Nano copper, the particle diameter of nano-particle of copper is 2 ~ 50nm.
In one embodiment, the caliber of described modified carbon nano-tube is 20 ~ 30nm.
Another aspect provides the preparation method Wu Ji – organic composite macromolecular flocculation agent, modified Nano copper, modified carbon nano-tube, POSS-MA-PEG and oil-based solvent are fully uniformly mixed by weight, and heat at 35 ~ 45 DEG C and be incubated 20 ~ 45min, to obtain final product.
In one embodiment, in described preparation method, temperature is 40 DEG C and is incubated 30min.
In one embodiment, described lubrication oil antiwear agent is used in lubricant products.
Below by embodiment, the present invention is specifically described.What be necessary to herein means out is; following examples are only for the invention will be further described; limiting the scope of the invention can not be interpreted as; some nonessential improvement and adjustment that the professional and technical personnel in this field makes according to the content of foregoing invention, still belong to protection scope of the present invention.
In addition, if do not have other to illustrate, raw materials used is all commercially available, and following material number used is weight part.
A1: (benzothiazole compound is modified Nano copper
)
A2: (benzothiazole compound is modified Nano copper
)
A3: (benzothiazole compound is modified Nano copper
)
A4: (benzothiazole compound is modified Nano copper
)
B1: modified carbon nano-tube
C1:POSS-MA-PEG(R is phenyl, and n is 70 ~ 130, R
1for amino)
C2:POSS-MA-PEG(R is phenyl, and n is 70 ~ 130, R
1for carboxyl)
C3:POSS-MA-PEG(R is cyclopentyl, and n is 70 ~ 130, R
1for amino)
D1：100N
Embodiment 1 ~ 8 and comparative example 1, comparative example 2 and comparative example 3:
Lubrication oil antiwear agent is prepared, preparation method's following (consumption of following component is parts by weight) according to the formula in table 1:
Modified Nano copper, modified carbon nano-tube, POSS-MA-PEG and oil-based solvent are fully uniformly mixed by weight, and heat at 40 DEG C and be incubated 30min, to obtain final product.
Table 1 is for preparing composition of raw materials and the consumption (parts by weight) of lubrication oil antiwear agent
Testing method:
(1) friction-wear test: according to GB314-82 standard, measures the lubrication oil antiwear agent in the above embodiment of the present invention and comparative example by four ball.Testing four-ball tester model used is MRS – 1J, and steel ball is secondary standard steel ball (GC15 bearing, HRC is 59-61), and rotating speed is 1480r/min, and temperature is room temperature.Lubrication oil antiwear agent is tested in SM10W-40 gasoline engine oil.
Above-mentioned test result is in table 2.Dosage in table 2 is the weight percentage that described lubrication oil antiwear agent accounts for SM10W-40 gasoline engine oil gross weight.
Table 2 is four ball evaluation results
As can be seen from above data, the lubrication oil antiwear agent of embodiment 1-8, in SM10W-40 gasoline engine oil, can improve the P of oil product effectively
bvalue, has good abrasion resistance.Compare with comparative example 3 with comparative example 1, comparative example 2, lubrication oil antiwear agent P of the present invention simultaneously
bgreatly, wear scar diameter is little, has good abrasion resistance.
(2) wear-resistant repairing performance test:
Tested by the wear-resistant machine (KMY201-1A type) of the dynamo-electric limited liability company in Divine Land, Wuhan, test philosophy is: on described wear-resistant machine, arrange rotor and stator, produce the friction surface of a wound by blank machine oil (not adding the machine oil of anti-wear agent), then add the lubrication oil antiwear agent that will test between the stator and the rotor and the surface of a wound is repaired.The mode of employing interpolation counterweight reinforcing increases the load between stators and rotators, seizing mutually during serious wear between stators and rotators, is characterized the wear-resistant repairing performance of lubrication oil antiwear agent thus by the weight of counterweight.
Use SP Series Gasoline Engines lubricating oil that sino-america joint-venture Beijing sunlight lubricating oil company limited produces as blank in this experiment, test the load that can carry, the lubrication oil antiwear agent of seizing rear embodiment adds in blank lubricating oil, the amount of lubrication oil antiwear agent is 3.5%, repair, run 30 seconds, test the load that can carry, the results are shown in Table 3.
Table 3 is the evaluation of rattling machine repairing performance
As can be seen from Table 3, the lubrication oil antiwear agent adding the embodiment of the present invention 1,3,6 can increase substantially the wear-resistant repairing performance of machine and the load of carrying.
Aforesaid example is only illustrative, for explaining some features of feature of the present invention.Appended claim is intended to the scope wide as far as possible that requirement it is contemplated that, and the embodiment presented herein is only the explanation of the embodiment of the selection of combination according to all possible embodiment.Therefore, the purpose of applicant is the selectional restriction that appended claim is not illustrated the example of feature of the present invention.And progress in science and technology is not replaced to be formed due to the inaccurate reason of language performance by the possible equivalent considered at present or son, and these changes also should be interpreted as being covered by appended claim in the conceived case.
Claims (10)
1. a lubrication oil antiwear agent, is characterized in that, described anti-wear agent is prepared from by comprising following raw material:
Modified Nano copper 100
Modified carbon nano-tube 36 ~ 60
POSS-MA-PEG20~55；
Described modified carbon nano-tube is the carbon nanotube of polyisobutene modification; The molecular structural formula of described POSS-MA-PEG is:
Wherein, R is the one in phenyl, isobutyl-, cyclopentyl and cyclohexyl, and n is 70 ~ 130, R
1for the one in hydroxyl, amino and carboxyl.
2. lubrication oil antiwear agent according to claim 1, is characterized in that, in described POSS-MA-PEG, R is phenyl or cyclopentyl.
3. lubrication oil antiwear agent according to claim 1, is characterized in that, in described raw materials, also comprise the oil-based solvent of 5 ~ 25 weight parts, described oil-based solvent is selected from one or more in various lubricating oil and base oil.
4. lubrication oil antiwear agent according to claim 1, is characterized in that, described modified Nano copper is the nano-particle of copper through benzothiazole compound in-situ-surface modifying.
5. lubrication oil antiwear agent according to claim 4, is characterized in that, described benzothiazole compound is selected from
In one.
6. lubrication oil antiwear agent according to claim 4, is characterized in that, in described modified Nano copper, the particle diameter of nano-particle of copper is 2 ~ 50nm.
7. lubrication oil antiwear agent according to claim 1, is characterized in that, the caliber of described modified carbon nano-tube is 20 ~ 30nm.
8. prepare the method for the lubrication oil antiwear agent in claim 1-7 described in any one, it is characterized in that, modified Nano copper, modified carbon nano-tube, POSS-MA-PEG and oil-based solvent are fully uniformly mixed by weight, and heat at 35 ~ 45 DEG C and be incubated 20 ~ 45min, to obtain final product.
9. the preparation method of lubrication oil antiwear agent according to claim 8, is characterized in that, in described preparation method, temperature is 40 DEG C and is incubated 30min.
10. one kind uses the lubricant products of the lubrication oil antiwear agent described in any one of claim 1 ~ 9.
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Cited By (2)
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| CN110272447A (en) * | 2018-03-17 | 2019-09-24 | 南京工业大学 | A method of preparing organosilicon Biolubrication oil base oil |
| CN116042293A (en) * | 2023-02-11 | 2023-05-02 | 道骐科技有限公司 | Multifunctional lubricating grease and preparation method thereof |
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| CN102174341A (en) * | 2011-04-01 | 2011-09-07 | 苏州之侨新材料科技有限公司 | Preparation method of carbon nano-tube/nano-copper compounded lubricating oil additive |
| CN103160077A (en) * | 2013-02-01 | 2013-06-19 | 厦门大学 | Self-lubrication-type wear-resistant epoxy resin containing POSS and preparation method thereof |
| CN104411770A (en) * | 2012-07-02 | 2015-03-11 | 贝克休斯公司 | Nanocomposite and method of making the same |
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| CN102174341A (en) * | 2011-04-01 | 2011-09-07 | 苏州之侨新材料科技有限公司 | Preparation method of carbon nano-tube/nano-copper compounded lubricating oil additive |
| CN104411770A (en) * | 2012-07-02 | 2015-03-11 | 贝克休斯公司 | Nanocomposite and method of making the same |
| CN103160077A (en) * | 2013-02-01 | 2013-06-19 | 厦门大学 | Self-lubrication-type wear-resistant epoxy resin containing POSS and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110272447A (en) * | 2018-03-17 | 2019-09-24 | 南京工业大学 | A method of preparing organosilicon Biolubrication oil base oil |
| CN110272447B (en) * | 2018-03-17 | 2021-11-12 | 南京工业大学 | Method for preparing organic silicon biological lubricating oil base oil |
| CN116042293A (en) * | 2023-02-11 | 2023-05-02 | 道骐科技有限公司 | Multifunctional lubricating grease and preparation method thereof |
| CN116042293B (en) * | 2023-02-11 | 2024-05-14 | 道骐科技有限公司 | Multifunctional lubricating grease and preparation method thereof |
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